Background technology
Poly-dextrose (Polydextrose claims again ID) is a kind of of water-soluble dietary fibre, is white or off-white color powdery solid, odorless, soluble in water, be at citric acid, under the existence of sorbyl alcohol, glucose high-temperature low-pressure reactive polymeric is formed to polymer, and its chemical formula is the polycondensate of the random bonding of glucose, but with 1,6-glycosidic link is combined into main D-Glucose polymer, be combined with a small amount of sorbyl alcohol, citric acid etc., molecular-weight average is greater than 3200, and mean polymerisation degree is greater than 20.Product form has A type, N-type, K type and modified polyglucose (Litesse) and refining poly-dextrose (II leqqeUltra) etc., A type is amorphous powder, white is to faint yellow, and 10% pH value of water solution is 2.5~3.5, during application, need regulate its acidity with buffer reagent; N-type is the aqueous solution of A type, colourless to faint yellow, concentration 70%, and pH value is neutralized to 5.0~6.0 with KOH; K type is to use food grade KHCO
3regulate poly-dextrose pH value of water solution to 5.0~6.0, then make solution is concentrated, dry, or with KOH, KHCO
3be dry mixed and form with A type powder; Poly-dextrose is carried out to catalytic hydrogenation processing and obtain white to milky modified polyglucose, the pH value of 10% aqueous solution is 3.0~4.5, acidity and bitter taste reduce, taste has larger improvement, refining the refining poly-dextrose forming is on this basis white solid, taste is salubrious, and the pH value of 10% solution is 4.5~6.5, solution colorless and odorless.
Poly-dextrose has whole intestines, regulates the effect of blood sugar and blood fat, can be used as foodstuff fibre widespread use in various functional foodstuffs.In addition, also there is following features:
Soluble dietary fibre poly-dextrose is a kind of polymer saccharide compound, belongs to food fibre category, has whole intestines, regulates the effect of blood sugar and blood fat, can be used as foodstuff fibre widespread use in various functional foodstuffs.
1. low in calories, without carious tooth
Poly-dextrose is a kind of material low in calories (4.148kJ/g), is about 1/4th of general carbohydrate (16.5kJ/g); Without carious tooth, difficult digested.
2. good water holding and water-retaining capacity
Poly-dextrose has good moisture retention, and its water activity is lower, can prevent or delay the variation of water content in food, contributes to control increase or the loss speed of moisture in food, by keeping moisture or preventing that water migration from extending the shelf-lives of product.
3. suitable viscosity
The viscosity of poly-dextrose solution is higher than the viscosity of same isoconcentration sucrose or Sorbitol Solution USP. when the carbohydrate in replacing food and fat, can form desirable mouthfeel.
4. correct freezing point
While using high-intensity sweetener to manufacture frozen food confection low in calories, can add the matrix that poly-dextrose is adjusted product, the matrix that compensation causes because granulated sugar reduces is lost, and improves because freezing point reduces the bad texture change causing.
5. good processing characteristics
Poly-dextrose stable in properties, good water solubility, compatibility scope is wide, in liquid and solid food, all can apply, and can be used in conjunction with numerous food supplementary materials.
Chinese patent No.90101110.X discloses a kind of by not preparing containing the poly-dextrose of low molecular organic acids the method that particle diameter is less than the powdery poly-dextrose of approximately 125 microns in fact.The method forms powdery poly-dextrose by grinding after the poly-dextrose that does not contain low molecular weight organic acid is mixed with anti-caking agent.China Patent No. No.03126106.X discloses a kind of poly-dextrose production technique and production equipment, adopts described process unit that the polymer content in poly-dextrose product is brought up to more than 90%; Reduced below the content to 4% of reducing sugar; Acidity and pH value are lower, and acidity is that 0.02, pH value reaches 5.Chinese patent application No.101824097 discloses a kind of production method of poly-dextrose, by adopting decolorizing resin adsorption bleaching after negative pressure polyreaction, then adopts dry the making of spraying.
Above-mentioned invention is all to make improvements on the process step of the production of poly-dextrose, artificial link is more, be unfavorable for that quality control and productive rate are lower, in sum, a kind of low cost is provided, the process for preparing poly-glucose that intelligent processing method, high yield and product stability are higher and relevant equipment are all the hot issues of the research of social needs instantly.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of production method and equipment of high purity Sugarless poly-glucose, by mechanical automation technology, improve existing production method in a plurality of links, improved greatly quality control and production and productivity and realized automatic continuous production; By intellectuality, control, can realize remote monitoring and the operation of whole system equipment; According to the requirement of actual production and equipment operation management, " four is distant " control of the remote signalling of feasible system, remote measurement, remote regulating, remote control.
The mouthfeel of poly-dextrose depends on the degree of the polyreaction in its preparation process, reacting mouthfeel more thorough and by product (as alditol) or the prepared poly-dextrose of unreacting material fewer (as sorbyl alcohol) will be better, and simultaneously the polymerization degree of poly-dextrose should be controlled between 16~30 to guarantee the Stability Analysis of Structures of poly-dextrose and not become grume and cannot enter follow-up treating process.For reaching above-mentioned object, contriver, through a large amount of research and experiment, has adjusted the production technique of poly-dextrose, has substantially obtained that preparation mouthfeel is good and low-cost, productive rate is high and product is stablized the production method of high poly-dextrose and relevant equipment.
One of the object of the invention is to provide a kind of production method of high purity Sugarless poly-glucose, comprises the following steps:
1) batching: get glucose, citric acid, Sorbitol Powder and prepare burden abundant mixing 85~95:0.1~1:5~15 by ratio of weight and the number of copies;
2) hot polymerization reaction: raw material drops into reactor at 170~190 ℃, stirring reaction 4-7 hour, keeping vacuum tightness is 0~-0.12MPa, in initial reaction stage, within 0.1~0.5 hour, keep normal pressure, then slowly adjust vacuum tightness, at polyreaction back segment, in the time of 4~6 hours, keep vacuum tightness higher than-0.085MPa, 0.5~1 hour last vacuum keep of polyreaction is-0.09~-0.12MPa; While closing on reaction end, by vacuum intake, adding concentration is that 1% edible alkali solution adjustment gained poly-dextrose pH value is 5.5-6;
3) cooling: after raw material is finished by reactor reaction, the poly-dextrose of molten state is uniformly distributed rear cooling;
4) film filter wash separation and purification: cooled poly-dextrose is soluble in water, make after the poly-dextrose solution of 10-30%, by the separation and purification of filtering membrane filter wash, the relative molecular weight of holding back of film is 400Da-900Da, and liquid and small-molecule substance penetrating fluid are held back in separation;
5) concentrated: gained feed liquid to be concentrated, to concentration 40-70%;
6) vacuum dehydrating at lower temperature: under vacuum state, feed liquid after concentrated is carried out to low temperature successive drying, obtain the Sugarless poly-glucose powder-product of white, mouthfeel free from extraneous odour, wherein keeping vacuum tightness is 0.07~0.12MPa, and temperature is 50~90 ℃.
Preferably, the molecular-weight average of the Sugarless poly-glucose that aforesaid method makes is 3500~4500Da, poly-dextrose content >=99%, glucose≤0.01%, 5-hydroxymethylfurfural≤0.006%, 1,6-dextrose anhydrous≤0.01%.
Preferably, after described adjustment pH value step, keep polyreaction to proceed 5~10 minutes.
Preferably, the hot polymerization reaction conditions in described step 2 is: temperature is that 175 ℃, stirring velocity are 650~700 revs/min.
Preferably, described edible alkali be sodium hydroxide, potassium hydroxide or with saleratus mixture.
Preferably, described edible alkali is that the ratio of weight and number of sodium hydroxide or potassium hydroxide and saleratus is 20-30:70-80.
Preferably, described filtering membrane is the organic rolled film of modification ether sulfone.
Two of the object of the invention is to provide a kind of production unit and system of high purity Sugarless poly-glucose, comprises reactor, refrigerating unit, vacuum unit, shredding unit, membrane filtration refining plant, vacuum and low temperature cooling and drying device and heat-conducting oil furnace.
Preferably, described system also comprises portioning machine.
The production method of high purity Sugarless poly-glucose provided by the invention and the beneficial effect of equipment and system are:
1. the vacuum tightness while adopting adjustment polyreaction is to guarantee the complete of polyreaction, the present invention is divided into three phases by the vacuum tightness of polyreaction: initial reaction stage keeps normal pressure, then slowly adjust vacuum tightness, two hours be not less than-0.085MPa of vacuum tightness in reaction later stage, remain on-0.09~-0.12MPa last half an hour.Polyreaction under vacuum tightness stage by stage produces that the product of gained is sparkling and crystal-clear, bright and mouthfeel is good.
2. reduce the pH value regulating step in existing production technique, it has been synchronizeed with polyreaction, improved production efficiency;
3. adopt vacuum and low temperature successive drying to replace conventional spray-drying tower, the yield of product greatly improves, and after employing Numeric Control Technology, the parameter of each equipment is more easily adjusted compared with spray-drying tower, and the preparation process stability and high efficiency of whole product and the stability of prepared Sugarless poly-glucose are promoted greatly.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention.Should be understood that following embodiment is only not used in and limits the scope of the invention for the present invention is described.The experimental technique of unreceipted actual conditions in the following example, conventionally according to normal condition, or the condition of advising according to manufacturer.Ratio and per-cent are based on weight, unless stated otherwise.
Production method of the present invention is to produce by following step the Sugarless poly-glucose that production method provided by the invention makes.
1. prepare burden
The parts by weight of take prepare material by glucose, sorbyl alcohol, citric acid in proportion as unit, and wherein glucose, citric acid, sorbyl alcohol, evenly mix.Also can adopt other formula rates as required, the even mixing of raw material guarantees the equilibrium of reaction, and wherein main raw material is glucose, and citric acid is catalyzer, and sorbyl alcohol is softening agent.
2. allocate 1% edible alkali solution
In dissolving vessel, inject 1800kgRO pure water.Open whipping appts, the 600kg poly-dextrose raw product of sloughing outer packaging is slowly poured in dissolving vessel.Then add water to dissolving vessel 5 ∕ 6 places, then get the sodium hydroxide of 0.25kg, be made into 10% sodium hydroxide solution, add slowly in dissolution kettle, be stirred well to solution clarification (approximately 40 minutes), then measure its pH value, keep its pH value 5.2 ± 0.1.Place standby.
3. hot polymerization reaction
The raw material mixing carries out polyreaction in reactor.It is 0~-0.12MPa that vacuum tightness is set in reaction, temperature of reaction is 170~180 ℃, reaction times is 4~7 hours, wherein vacuum tightness is divided three phases adjustment: initial reaction stage keeps normal pressure, then slowly adjust vacuum tightness, two hours be not less than-0.085MPa of vacuum tightness in reaction later stage, remain on-0.09~-0.1MPa(last half an hour and open the front first boiled water pipe of vacuum, then drive motor).Reaction vacuum tightness, temperature of reaction, reaction times also can adopt other suitable conditions.Reactor can adopt high temperature interlayer stainless steel cauldron, or the reactor of other similar purposes.By heat-conducting oil furnace, circulate and keep temperature of reaction.
Before production, first carry out pre-heating temperature elevation, then start reactor, after temperature reaches necessarily, start to feed intake, divide and finish for three times, the rear grade that fed intake is opened vacuum system for 20 minutes.When reaction closes on and finishes, by vacuum, feed intake to the edible alkali solution solution that adds 1% in reactor, after stirring, continuing reaction, within 5~10 minutes, to record pH value be that 5.5~6 rear end are reacted.The product color of gained should be yellow translucent body, pool bright, compared with thickness, more thickness explanation level of response is better.
4. cooling
By in the completely reacted poly-dextrose crude product access refrigerating unit that cleaning and sterilization has been crossed in advance, open the following baiting valve of reactor, the poly-dextrose crude product of gained just flows into refrigerating unit, the rapid grumeleuse of product of polyreaction gained is also sent to refrigerating unit tail end, is then delivered to the temporary tank of material.
5. pulverize
Before pulverizing, first the alcohol with 75% carries out spray disinfectant to pulverizer stainless steel mesh and food contact surface.Wait for about 10 minutes, treat its seasoning.Install 80 order stainless steel meshs.Open pulverizer power supply, then open the motor under the temporary tank of material, the mass transport in the temporary tank of material is pulverized to pulverizer.
6. decolouring
Poly-dextrose after dissolving is decoloured and processed as ion-exchange or gac through ordinary method, make solution whiteness reach 85-95%.
7. membrane filtration
Dissolving or the liquid poly-dextrose solution after decolouring are circulated through membrane filtration, and further to reduce the impurity of product, the concentrated fluid cylinder of liquid inflow after concentrating, specifically adopts the organic rolled film of modification ether sulfone to filter.
8. evaporation concentration
It is 40~70% that concentrated solution through in the concentrated fluid cylinder of being stored in of membrane filtration is further concentrated into concentration by triple effect thickening equipment, wherein under meter is controlled to 10~15LPM, makes product more be conducive to carry out vacuum-drying.
9. vacuum dehydrating at lower temperature
Adopt vacuum dehydrating at lower temperature to substitute conventionally spray-dried tower and be dried, be specially: using a continous vacuum low temperature drying system is 0.07~0.12MPa in vacuum tightness, temperature is at 50~90 ℃, to carry out successive drying.
Comparative example
Proportioning raw materials adopts 85 parts of glucose, 1.5 parts of citric acids, 5 parts of sorbyl alcohols, mixes.
The raw material mixing polymerization in reactor, it is normal pressure that reaction starts in 30 minutes, follow-up slow adjustment vacuum tightness, 2 hours vacuum tightnesss in reaction later stage are-0.085MPa to react last 30 minutes be adjusted into-0.1MPa; 170 ℃ of temperature of reaction, react after 4 hours and stop.Reactor adopts high temperature interlayer stainless steel cauldron, by heat-conducting oil furnace, is circulated and is kept temperature of reaction.
Under material in reactor molten state, regulate rapidly pH value.Use 1% sodium hydroxide to be adjusted to pH5.5.Regulate after pH value, continue to stir 5 minutes.
It is dry that reaction finishes above-mentioned cooling, the pulverizing of rear employing, membrane filtration, evaporation concentration and conventional spray-drying tower.
Obtain refined powder powder Sugarless poly-glucose product, detect each index of products obtained therefrom, concrete detected result is in Table 1.
Embodiment 1
Proportioning raw materials adopts 95 parts of glucose, 0.1 part of citric acid, 5 parts of sorbyl alcohols, mixes.
The raw material mixing polymerization in reactor, it is normal pressure that reaction starts in 30 minutes, follow-up slow adjustment vacuum tightness, 2 hours vacuum tightnesss in reaction later stage are 0.09MPa, react last 30 minutes be adjusted into-0.12MPa; 180 ℃ of temperature of reaction, react after 7 hours and stop.Reactor adopts high temperature interlayer stainless steel cauldron, by heat-conducting oil furnace, is circulated and is kept temperature of reaction.
Under material in reactor molten state, regulate rapidly pH value.Use 1% potassium hydroxide to be adjusted to pH6.Regulate after pH value, continue to stir 5 minutes.
Reaction finish above-mentioned cooling, the pulverizing of rear employing, membrane filtration, evaporation concentration and vacuum dehydrating at lower temperature (70 ℃, 0.10MPa) obtain refined powder powder Sugarless poly-glucose product, detect each index of products obtained therefrom, concrete detected result is in Table 1.
Embodiment 2
Proportioning raw materials adopts 90 parts of glucose, 1 part of citric acid, 9.5 parts of sorbyl alcohols, mixes.
The raw material mixing polymerization in reactor, it is normal pressure that reaction starts in 30 minutes, follow-up slow adjustment vacuum tightness, 2 hours vacuum tightnesss in reaction later stage are-0.09MPa to react last 30 minutes be adjusted into-0.11MPa; 175 ℃ of temperature of reaction, react after 5 hours and stop.Reactor adopts high temperature interlayer stainless steel cauldron, by heat-conducting oil furnace, is circulated and is kept temperature of reaction.
Under material in reactor molten state, regulate rapidly pH value.Use 1% sodium hydroxide and saleratus mixed solution (weight ratio is 20:80) to be adjusted to pH5.Regulate after pH value, continue to stir 5 minutes.
Reaction finish above-mentioned cooling, the pulverizing of rear employing, membrane filtration, evaporation concentration and vacuum dehydrating at lower temperature (90 ℃, 0.07MPa) obtain refined powder powder Sugarless poly-glucose product, detect each index of products obtained therefrom, concrete detected result is in Table 1.
Embodiment 3
Proportioning raw materials adopts 90 parts of glucose, 1 part of citric acid, 9.5 parts of sorbyl alcohols, mixes.
The raw material mixing polymerization in reactor, it is normal pressure that reaction starts in 30 minutes, follow-up slow adjustment vacuum tightness, 2 hours vacuum tightnesss in reaction later stage are-0.09MPa to react last 30 minutes be adjusted into-0.11MPa; 175 ℃ of temperature of reaction, react after 5 hours and stop.Reactor adopts high temperature interlayer stainless steel cauldron, by heat-conducting oil furnace, is circulated and is kept temperature of reaction.
Under material in reactor molten state, regulate rapidly pH value.Use 1% potassium hydroxide and saleratus mixed solution (weight ratio is 30:70) to be adjusted to pH5.Regulate after pH value, continue to stir 5 minutes.
Reaction finish above-mentioned cooling, the pulverizing of rear employing, membrane filtration, evaporation concentration and vacuum dehydrating at lower temperature (60 ℃, 0.09MPa) obtain refined powder powder Sugarless poly-glucose product, detect each index of products obtained therefrom, concrete detected result is in Table 1.
Embodiment 4
Proportioning raw materials adopts 89 parts of glucose, 1 part of citric acid, 10 parts of sorbyl alcohols, mixes.
The raw material mixing polymerization in reactor, it is normal pressure that reaction starts in 30 minutes, follow-up slow adjustment vacuum tightness, 2 hours vacuum tightnesss in reaction later stage are-0.85MPa to react last 30 minutes be adjusted into-0.10MPa; 175 ℃ of temperature of reaction, react after 4 hours and stop.Reactor adopts high temperature interlayer stainless steel cauldron, by heat-conducting oil furnace, is circulated and is kept temperature of reaction.
Under material in reactor molten state, regulate rapidly pH value.Use 1% sodium hydroxide and saleratus mixed solution (weight ratio is 20:70) to be adjusted to pH5.Regulate after pH value, continue to stir 5 minutes.
Reaction finish above-mentioned cooling, the pulverizing of rear employing, membrane filtration, evaporation concentration and vacuum dehydrating at lower temperature (50 ℃, 0.12MPa) obtain refined powder powder Sugarless poly-glucose product, detect each index of products obtained therefrom, concrete detected result is in Table 1.
Table 1
As shown in table 1 result, in Sugarless poly-glucose preparation method provided by the invention, the polymeric reaction condition of gained poly-dextrose the best is: proportioning raw materials adopts 89 parts of glucose, 1 part of citric acid, 10 parts of sorbyl alcohols, polymerization in reactor after mixing, it is normal pressure that reaction starts in 30 minutes, follow-up slow adjustment vacuum tightness, 2 hours vacuum tightnesss in reaction later stage are-0.85MPa to react last 30 minutes be adjusted into-0.10MPa; 175 ℃ of temperature of reaction, react after 4 hours and stop, and adopt the drying loss of vacuum dehydrating at lower temperature to be starkly lower than traditional conventional spray-drying tower.